WO2021147295A1 - 电池用粘合剂、锂离子电池负极片以及锂离子电池 - Google Patents

电池用粘合剂、锂离子电池负极片以及锂离子电池 Download PDF

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WO2021147295A1
WO2021147295A1 PCT/CN2020/106529 CN2020106529W WO2021147295A1 WO 2021147295 A1 WO2021147295 A1 WO 2021147295A1 CN 2020106529 W CN2020106529 W CN 2020106529W WO 2021147295 A1 WO2021147295 A1 WO 2021147295A1
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battery
acrylate
hydrophilic
methacrylate
binder
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English (en)
French (fr)
Chinese (zh)
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潘中来
张晓正
陶伟
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Meishan Indigo Technology Co Ltd
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Meishan Indigo Technology Co Ltd
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Priority to EP20915776.7A priority Critical patent/EP4095213A4/en
Priority to KR1020227028830A priority patent/KR102947827B1/ko
Priority to JP2022544430A priority patent/JP7480310B2/ja
Priority to US17/794,258 priority patent/US20230068865A1/en
Publication of WO2021147295A1 publication Critical patent/WO2021147295A1/zh
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    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
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    • C08F220/26—Esters containing oxygen in addition to the carboxy oxygen
    • C08F220/28—Esters containing oxygen in addition to the carboxy oxygen containing no aromatic rings in the alcohol moiety
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    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Definitions

  • the invention relates to a binder for a battery, a negative electrode sheet of a lithium ion battery and a lithium ion battery, and belongs to the technical field of lithium ion batteries.
  • lithium-ion batteries As the most ideal mobile power source, lithium-ion batteries have the incomparable advantages of high energy density, small size, long life, and no pollution. They are widely used in electric vehicles, aerospace, communications, and various portable electrical appliances.
  • Lithium-ion batteries are mainly composed of electrode sheets (including positive electrode sheets and negative electrode sheets), separators, and electrolyte.
  • the electrode sheets are all composed of electrode active material powder, binder, conductive agent and current collector.
  • the electrode active material, conductive agent, and binder solution are usually mixed and ground uniformly to form a slurry, and then coated on the copper foil or aluminum foil as the current collector, and then dried and rolled. Wait for the process to get. It can be seen that the adhesive plays a key role in the preparation of the electrode sheet.
  • the water-based adhesive has the advantages of safety, pollution-free, no need to recycle solvents, simple operation, etc., making it the first choice for electrode adhesives for lithium-ion batteries.
  • commonly used water-based adhesives are SBR (styrene butadiene rubber emulsion), LA132, LA133 and so on.
  • the SBR water-based binder uses water as the dispersion medium of the negative electrode active material powder, which is environmentally friendly, non-polluting, and harmful to production operators.
  • SBR is used as a binder for the anode active material powder of lithium-ion batteries, and the overall performance of the battery can no longer meet the application requirements of increasing battery quality.
  • the technical problem solved by the present invention is to provide a battery adhesive with strong adhesion.
  • the battery binder of the present invention contains a water-soluble polymer with both hydrophilic and hydrophobic units; and in the polymer, the low- and medium-molecular-weight polymer accounts for less than 5 wt% of the total polymer.
  • the molecular weight of the molecular weight polymer is less than or equal to 100,000.
  • the weight percentage of hydrophilic units and hydrophobic units in the polymer is 30-70%:70-30%.
  • the weight percentage of the hydrophilic unit and the hydrophobic unit is 40-60%:60-40%.
  • the low- and medium-molecular-weight polymer accounts for less than 2% of the total polymer. In a specific embodiment, the low to medium molecular weight polymer accounts for less than 1% of the total polymer.
  • the low molecular weight polymer accounts for less than 0.5 wt% of the total polymer, and the molecular weight of the low molecular weight polymer is less than or equal to 50,000.
  • the hydrophilic unit contains a carboxyl group or a sulfonic acid group.
  • the hydrophobic unit is introduced by a lipophilic monomer
  • the hydrophilic unit is introduced by a hydrophilic monomer
  • R 2 is selected from -CN, -C 6 H 5 , -COOCH 3 , -COOCH 2 CH 3 , -COOCH 2 CH 2 CH 2 CH 3 , -COOC(CH 3 ) 3 , -COOCH 2 CH(CH 2 CH 3 )CH 2 CH 2 CH 2 CH 3 , -COOC 12 H 25 , -COO(CH 2 ) 17 CH 3 ⁇ COOCH 2 CH 2 OH, ⁇ OCOCH 3 or
  • the lipophilic monomer is acrylonitrile, methacrylonitrile, styrene, methyl acrylate, ethyl acrylate, n-butyl acrylate, t-butyl acrylate, 2-ethylhexyl acrylate Ester, cyclohexyl acrylate, isobornyl acrylate, hydroxyethyl acrylate, hydroxypropyl acrylate, vinyl acetate, methacrylonitrile, methyl methacrylate, ethyl methacrylate, n-butyl methacrylate, At least one of 2-ethylhexyl methacrylate, cyclohexyl methacrylate, isobornyl methacrylate, hydroxyethyl methacrylate, hydroxypropyl methacrylate, and glycidyl methacrylate Species; the hydrophilic monomers include acrylic acid, acrylate, methacrylate, methacryl
  • hydrophilic monomers also include acrylamide, N-methacrylamide, N-ethylacrylamide, N,N-dimethylacrylamide, N,N-diethylacrylamide, 2 -At least one of methacrylamide, N-methylolacrylamide, N-hydroxyethyl acrylamide, and N-hydroxypropyl acrylamide.
  • the lipophilic monomers are acrylonitrile and butyl acrylate, and the hydrophilic monomers are acrylic acid, N-vinylpyrrolidone and acrylamide.
  • the lipophilic monomers are methacrylonitrile, methyl acrylate and hydroxypropyl acrylate, and the hydrophilic monomers are methacrylic acid and N-methacrylamide.
  • the lipophilic monomer is 2-ethylhexyl acrylate, cyclohexyl methacrylate and ethyl methacrylate
  • the hydrophilic monomer is 2-acrylamide-2-methyl Propanesulfonic acid, N,N-diethylacrylamide and itaconate.
  • the lipophilic monomers are ethyl acrylate, vinyl acetate and hydroxyethyl methacrylate
  • the hydrophilic monomers are acrylate, 2-methacrylamide and vinyl sulfonic acid. Salt.
  • the lipophilic monomer is styrene, 2-ethylhexyl methacrylate and hydroxypropyl methacrylate, and the hydrophilic monomer is maleic acid, N-vinylpyrrolidone and N-hydroxypropyl acryl.
  • the lipophilic monomers are 2-ethylhexyl acrylate, ethyl acrylate and isobornyl methacrylate, and the hydrophilic monomers are acrylic acid, methacrylic acid, and N-hydroxyethyl. Acrylic and acrylic acid.
  • the weight percentage of hydrophilic monomers and lipophilic monomers is 30-70%:70-30%. In some embodiments, the weight percentage of hydrophilic monomers and lipophilic monomers is 40-60%:60-40%.
  • the binder for batteries further includes a solvent
  • the solvent is an organic solvent or water.
  • the solvent is water.
  • the pH value of the adhesive whose solvent is water is 6-12; in some embodiments, the pH value of the adhesive whose solvent is water is 6.5-9.
  • the battery binder further contains additives, and the additives include at least one of a dispersant, a leveling wetting agent, a defoaming agent, and a softening agent.
  • the present invention also provides a method for preparing a battery binder whose solvent is water.
  • the preparation method of the adhesive for batteries includes the following steps: heating the hydrophilic monomer, lipophilic monomer and water to the reaction temperature in a protective atmosphere, adding an initiator to initiate the reaction, and obtaining a solid-liquid mixture, and then taking Precipitate and neutralize to obtain a binder for batteries.
  • the present invention also provides the application of the battery binder of the present invention in the preparation of the negative electrode sheet of the lithium ion battery.
  • the present invention also provides the application of the battery binder of the present invention in the preparation of lithium ion battery pole pieces.
  • the adhesive for batteries of the present invention has high adhesive force and can be used in the preparation of lithium ion battery pole pieces to improve battery performance.
  • the invention also provides a lithium ion battery negative electrode sheet.
  • the lithium ion battery negative electrode sheet of the present invention includes a negative electrode active material and a binder, wherein the binder is the battery binder of the present invention.
  • the invention also provides a lithium ion battery.
  • the lithium ion battery of the present invention includes a positive electrode, a negative electrode and an electrolyte, wherein the negative electrode is the negative electrode sheet of the lithium ion battery of the present invention.
  • the present invention also provides a battery pack, which includes a plurality of batteries according to the present invention.
  • the present invention has the following beneficial effects:
  • the adhesive of the present invention has strong adhesive force, simple preparation method and low cost. Compared with the conventional negative electrode sheet binder of 2.5 to 5%, when the binder of the present invention is used at 1.5 to 2%, it is not only It can show higher adhesion and increase the proportion of active material (negative electrode material), thereby increasing the energy density of the battery.
  • Figure 1 shows the molecular weight test results of the adhesives of Example 1 and Comparative Example 1 of the present invention.
  • Figure 2 shows the cycle performance of batteries prepared using the binders of Example 1 and Comparative Examples 1 and 2 of the present invention.
  • Figure 3 shows the low-temperature discharge results of batteries prepared using the binders of Example 1 and Comparative Examples 1 and 2 of the present invention.
  • the hydrophilic monomers exist in the form of acid or salt in water, but when they exist in the form of acid, their hydrophilicity is low. If the monomers of the polymerization reaction are copolymerized in the water phase with a composition of low hydrophilicity, the reaction product will precipitate out due to insufficient hydrophilicity, forming a mixture of water, residual monomers and precipitates.
  • the polymerization reaction is terminated, which will greatly reduce the formation of low- and medium-molecular-weight polymers, and further separate the precipitate by physical means, leaving unreacted monomers and a small amount of low- and medium-molecular-weight polymers in the reaction system (water In phase), the precipitate is a high-molecular-weight polymer, and the content of low- and medium-molecular-weight polymer in the precipitate is relatively low.
  • the polymer can be directly dissolved in organic solvents such as NMP and used as a binder, or it can be neutralized or hydrolyzed by adding alkali After improving the hydrophilicity of the copolymer, the copolymer is uniformly dispersed in the water phase to obtain an aqueous adhesive.
  • the mechanical properties such as cohesion and adhesion of the obtained adhesive are significantly improved, so that the adhesive prepared by the precipitation has better bonding performance, and further reduces the adhesive The dosage can improve battery performance.
  • the battery binder of the present invention includes a polymer with both a hydrophilic unit and a hydrophobic unit; and in the polymer, the low- and medium-molecular-weight polymer accounts for less than 5 wt% of the total polymer.
  • the molecular weight of low-molecular-weight polymers is less than or equal to 100,000.
  • the battery binder of the present invention includes a polymer with both a hydrophilic unit and a hydrophobic unit; and in the polymer, a medium-low molecular weight polymer accounts for less than 5 wt% of the total polymer.
  • the medium-low molecular weight polymer The molecular weight is less than or equal to 100,000.
  • control the medium and low molecular weight polymers to account for 0.5wt%, 0.8wt%, 1wt%, 1.5wt%, 2wt%, 2.5wt%, 3wt%, 3.5wt%, 4wt%, 4.5 of the total polymer wt%, 5wt%, etc.
  • the weight percentage of hydrophilic units and hydrophobic units in the polymer is 30-70%:70-30%.
  • the weight percentages of hydrophilic units and hydrophobic units in the polymer are 30%: 70%, 35%: 65%, 40%: 60%, 42%: 58%, 45%: 55%, 47%. %: 53%, 50%: 50%, 51%: 49%, 55%: 45%, 58%: 42%, 60%: 40%, etc.
  • the weight percentage of the hydrophilic unit and the hydrophobic unit is 40-60%:60-40%.
  • the low to medium molecular weight polymer accounts for less than 2% of the total polymer. In a specific embodiment, the low-to-medium molecular weight polymer accounts for less than 1% of the total polymer.
  • the low-molecular-weight polymer accounts for less than 0.5 wt% of the total polymer, and the molecular weight of the low-molecular-weight polymer is ⁇ 50,000.
  • the low molecular weight polymer is controlled to account for 0.1 wt%, 0.2 wt%, 0.3 wt%, 0.4 wt%, 0.5 wt%, etc. of the total polymer.
  • the molecular weights mentioned in the present invention are all weight average molecular weights (Mw).
  • the medium and low molecular weight polymers of the present invention are polymers with a molecular weight of ⁇ 100,000.
  • the low-molecular-weight polymer of the present invention is a polymer with a molecular weight of less than 50,000.
  • the polymer is an amphiphilic copolymer, and the hydrophilic unit contains a carboxyl group or a sulfonic acid group.
  • the hydrophobic unit of the polymer is introduced by a lipophilic monomer, and the hydrophilic unit is introduced by a hydrophilic monomer, and the hydrophilic monomer contains a carboxyl group or a sulfonic acid group.
  • the amphiphilic polymer of the present invention can be obtained by copolymerizing a lipophilic monomer and a hydrophilic monomer.
  • R 1 is selected from -H or -CH 3 ;
  • R 2 is selected from ⁇ CN, ⁇ C 6 H 5 , ⁇ COOCH 3 , ⁇ COOCH 2 CH 3 , ⁇ COOCH 2 CH 2 CH 2 CH 3 , -COOC(CH 3 ) 3 , ⁇ COOCH 2 CH(CH 2 CH 3 )CH 2 CH 2 CH 2 CH 3 ⁇ -COOC 12 H 25 ⁇ -COO(CH 2 ) 17 CH 3 ⁇ COOCH 2 CH 2 OH, ⁇ COOCH 3 CHCH 2 OH, ⁇ COOCH 2 CHOHCH 3 , ⁇ OCOCH 3 or
  • R 3 is selected from -H, -CH 3 or -COOM 1 ;
  • M 1 includes H, Li, Na, K, Ca, Zn or Mg;
  • R 4 is selected from -H, -CH 3 or -COOM 2 ;
  • M 2 includes H, Li, Na, K, Ca, Zn or Mg;
  • R 5 is selected from ⁇ COOM 3 , ⁇ CH 2 COOM 3 , ⁇ COO(CH 2 ) 6 SO 3 M 3 , ⁇ CONH 2 , ⁇ CONHCH 3 , ⁇ CONHCH 2 CH 3 , ⁇ CON(CH 3 ) 2 , ⁇ CON(CH 2 CH 3 ) 2 , ⁇ CH2CHCONHCH 2 OH, ⁇ CH 2 CHCONHCH 2 CH 2 OH, ⁇ CONHC(CH 3 ) 2 CH 2 SO 3 H , -CH 2 SO 3 M or M 3 includes H, Li, Na, K, Ca, Zn, or Mg.
  • R 2 is selected from -CN, -C 6 H 5 , -COOCH 3 , -COOCH 2 CH 3 , -COOCH 2 CH 2 CH 2 CH 3 , -COOC(CH 3 ) 3 , -COOCH 2 CH(CH 2 CH 3 )CH 2 CH 2 CH 2 CH 3 , -COOC 12 H 25 , -COO(CH 2 ) 17 CH 3 ⁇ COOCH 2 CH 2 OH, ⁇ OCOCH 3 or
  • the lipophilic monomer includes acrylonitrile, methacrylonitrile, styrene, methyl acrylate, ethyl acrylate, n-butyl acrylate, t-butyl acrylate, 2-ethylhexyl acrylate , Cyclohexyl acrylate, isobornyl acrylate, hydroxyethyl acrylate, hydroxypropyl acrylate, vinyl acetate, methacrylonitrile, methyl methacrylate, ethyl methacrylate, n-butyl methacrylate, methyl methacrylate At least one of 2-ethylhexyl acrylate, cyclohexyl methacrylate, isobornyl methacrylate, hydroxyethyl methacrylate, hydroxypropyl methacrylate, and glycidyl methacrylate .
  • the hydrophilic monomers include acrylic acid, acrylate, methacrylic acid, methacrylate, allyloxy hydroxypropyl sulfonic acid, allyloxy hydroxypropyl sulfonate, vinyl sulfonic acid, vinyl Sulfonate, 2-acrylamide-2-methylpropanesulfonic acid, propylene sulfonic acid, propylene sulfonate, methacrylic acid, methacrylic acid salt, N-vinylpyrrolidone, itaconic acid, coat At least one of konate, maleic acid, and maleate.
  • hydrophilic unit contains a carboxyl group or a sulfonic acid group, it is necessary to ensure that at least one hydrophilic monomer contains a carboxyhusulphonic acid group.
  • Monomers containing carboxyl or sulfonic acid groups can be adjusted for hydrophilicity to ensure that the polymer precipitates in water and becomes a salt form after adding lye, thereby enhancing the hydrophilicity and dissolving in water.
  • the hydrophilic monomer also includes acrylamide, N-methacrylamide, N-ethylacrylamide, N,N-dimethylacrylamide, N,N- At least one of diethylacrylamide, 2-methacrylamide, N-methylolacrylamide, N-hydroxyethyl acrylamide, and N-hydroxypropyl acrylamide.
  • the introduction of these amide hydrophilic monomers can provide other functions.
  • the polymer in the adhesive of the present invention is formed by copolymerizing at least one hydrophilic monomer and at least one lipophilic monomer.
  • the polymer is formed by copolymerizing a lipophilic monomer and a hydrophilic monomer.
  • the lipophilic monomer is acrylonitrile, and the hydrophilic monomer is acrylic acid.
  • the lipophilic monomer is methacrylonitrile, and the hydrophilic monomer is methacrylic acid.
  • the lipophilic monomer is hydroxyethyl acrylate, and the hydrophilic monomer is vinyl sulfonate.
  • the lipophilic monomer is cyclohexyl methacrylate, and the hydrophilic monomer is methacrylate.
  • the lipophilic monomer is vinyl acetate, and the hydrophilic monomer is methacrylic acid.
  • the lipophilic monomer is glycidyl methacrylate, and the hydrophilic monomer is itaconic acid.
  • the lipophilic monomer is 2-ethylhexyl acrylate, and the hydrophilic monomer is maleic acid.
  • the lipophilic monomer is hydroxyethyl methacrylate, and the hydrophilic monomer is vinyl sulfonic acid.
  • the lipophilic monomer is methacrylonitrile, and the hydrophilic monomer is 2-acrylamide-2-methylpropanesulfonic acid.
  • the lipophilic monomer is styrene, and the hydrophilic monomer is propylene sulfonic acid.
  • the lipophilic monomer is methyl acrylate, and the hydrophilic monomer is allyloxy hydroxypropyl sulfonic acid.
  • the lipophilic monomer is tert-butyl acrylate, and the hydrophilic monomer is methacrylic acid salt.
  • the polymer in the adhesive of the present invention is formed by copolymerizing a lipophilic monomer and a plurality of hydrophilic monomers.
  • the lipophilic monomer is acrylonitrile
  • the hydrophilic monomer is acrylic acid and methacrylic acid.
  • the lipophilic monomer is acrylonitrile
  • the hydrophilic monomer is acrylic acid and acrylamide.
  • the lipophilic monomer is methacrylonitrile
  • the hydrophilic monomer is acrylate, methacrylic acid, and N-methacrylamide.
  • the lipophilic monomer is styrene, and the hydrophilic monomer is acrylic acid, acrylate, methacrylic acid, methacrylate, and acrylamide.
  • the lipophilic monomer is methyl acrylate, and the hydrophilic monomer is vinylsulfonic acid, 2-acrylamide-2-methylpropanesulfonic acid, and itaconic acid.
  • the lipophilic monomer is and the hydrophilic monomer is.
  • the lipophilic monomer is n-butyl methacrylate, and the hydrophilic monomer is acrylic acid, acrylate and acrylamide.
  • the lipophilic monomer is tert-butyl acrylate, and the hydrophilic monomer is N,N-dimethylacrylamide, 2-methacrylamide, and maleic acid.
  • the lipophilic monomer is acrylonitrile, and the hydrophilic monomer is acrylate, methacrylic acid, methacrylate, acrylamide, N-methacrylamide, and N-ethylacrylamide.
  • the polymer in the adhesive of the present invention is copolymerized with a variety of lipophilic monomers and a hydrophilic monomer.
  • the lipophilic monomer is acrylonitrile, methacrylonitrile, styrene and methyl acrylate
  • the hydrophilic monomer is acrylic acid.
  • the lipophilic monomer is styrene, methyl acrylate, ethyl acrylate, and t-butyl acrylate
  • the hydrophilic monomer is methacrylic acid.
  • the lipophilic monomer is vinyl acetate, methacrylonitrile, methyl methacrylate, and ethyl methacrylate, and the hydrophilic monomer is allyloxy hydroxypropyl sulfonic acid.
  • the lipophilic monomer is cyclohexyl methacrylate, isobornyl methacrylate, and glycidyl methacrylate, and the hydrophilic monomer is maleic acid.
  • the lipophilic monomer is styrene, methyl acrylate, and hydroxypropyl acrylate, and the hydrophilic monomer is itaconic acid.
  • the lipophilic monomer is, and the hydrophilic monomer is allyloxy hydroxypropyl sulfonic acid.
  • the lipophilic monomer is hydroxypropyl acrylate, vinyl acetate, methacrylonitrile and methyl methacrylate, and the hydrophilic monomer is vinyl sulfonic acid.
  • the lipophilic monomer is styrene, methacrylonitrile, methyl methacrylate, and isobornyl methacrylate, and the hydrophilic monomer is propylene sulfonic acid.
  • the polymer in the adhesive of the present invention is copolymerized by a variety of lipophilic monomers and a variety of hydrophilic monomers.
  • the lipophilic monomers are acrylonitrile and butyl acrylate
  • the hydrophilic monomers are acrylic acid, N-vinylpyrrolidone and acrylamide.
  • the lipophilic monomers are methacrylonitrile, methyl acrylate and hydroxypropyl acrylate
  • the hydrophilic monomers are methacrylic acid and N-methacrylamide.
  • the lipophilic monomer is 2-ethylhexyl acrylate, cyclohexyl methacrylate and ethyl methacrylate
  • the hydrophilic monomer is 2-acrylamide-2-methyl Propanesulfonic acid, N,N-diethylacrylamide and itaconate.
  • the lipophilic monomers are ethyl acrylate, vinyl acetate and hydroxyethyl methacrylate
  • the hydrophilic monomers are acrylate, 2-methacrylamide and vinyl sulfonic acid. Salt.
  • the lipophilic monomer is styrene, 2-ethylhexyl methacrylate and hydroxypropyl methacrylate, and the hydrophilic monomer is maleic acid, N-vinylpyrrolidone and N-hydroxypropyl acryl.
  • the lipophilic monomers are 2-ethylhexyl acrylate, ethyl acrylate and isobornyl methacrylate, and the hydrophilic monomers are acrylic acid, methacrylic acid, and N-hydroxyethyl. Acrylic and acrylic acid.
  • the weight percentage of hydrophilic monomers and lipophilic monomers is 30-70%:70-30%.
  • the weight percentage of hydrophilic monomer and lipophilic monomer is 40-60%:60-40%.
  • the weight percentage of hydrophilic monomer and lipophilic monomer is 40%:60%; as another specific embodiment, the weight percentage of hydrophilic monomer and lipophilic monomer As another specific embodiment, the weight percentage of the hydrophilic monomer and lipophilic monomer is 50%:50%; as another specific embodiment, the hydrophilic monomer The weight percentage of lipophilic monomer is 55%:45%; as another specific embodiment, the weight percentage of hydrophilic monomer and lipophilic monomer is 60%:40%, etc.
  • the adhesive for the battery of the present invention as a product, can be solid, and can be used after adding a solvent to make it a glue during use, or can be a liquid product for direct use.
  • the binder for batteries further includes a solvent
  • the solvent is an organic solvent or water.
  • Organic solvents commonly used in this field are suitable for the present invention, such as NMP and the like.
  • the solvent is water. Adhesives that use water as solvent have the advantages of being safe, pollution-free, no need to recycle solvents, and simple operation.
  • the pH of the adhesive is 6-12.
  • the pH value is 6-12, the polymer mostly exists in the form of ionic polymer, which can increase its hydrophilic ability, so that it can be dissolved in water well.
  • the pH value can be adjusted by conventional methods.
  • lye is added to adjust the pH value.
  • the lye is an alkali metal hydroxide, such as sodium hydroxide solution, potassium hydroxide solution, etc., or sodium carbonate, Alkaline solutions such as ammonia or organic amines.
  • sodium hydroxide solution is used to adjust the pH.
  • the pH of the adhesive is 6.5-9.
  • the binder for batteries of the present invention is composed only of polymer and water, and there are no other additives in the binder.
  • the binder for a battery further contains an additive, and the additive includes at least one of a dispersant, a leveling wetting agent, a defoaming agent, and a softening agent.
  • the amount of these additives is the conventional amount in the field, for example, the additive content is less than 5% of the total weight of the water-based adhesive. In some specific embodiments, the content of the additives is 3% or less, 1% or less, 0.5% or less, 0.1% or less, 0% or the like of the total weight of the adhesive.
  • the dispersant can be an anionic dispersant such as oleate, sulfonate, carboxylate, etc., or a cationic dispersant such as ammonium salt, quaternary ammonium salt, pyridine salt, etc., or non-ionic dispersant.
  • Agents such as polyethers, acetylene glycols, CMC, etc., can also be supramolecular dispersants such as phosphate ester type high molecular polymers.
  • the leveling and wetting agent is a high boiling point solvent such as alcohols, ketones, esters or multifunctional high boiling point solvent mixtures, which can be long-chain resins such as acrylics, fluorocarbon resins, etc., or silicones Such as diphenyl polysiloxane, methyl phenyl polysiloxane and so on.
  • the defoaming agent can be organic small molecule alcohols or ethers such as ethanol, isopropanol, butanol, etc., or can be silicones, polyethers, such as polydimethylsiloxane, pentaerythritol ether, and the like.
  • Softeners are water-soluble organic solvents such as ethanol, propylene glycol, butylene glycol, glycerin, dimethyl sulfoxide, etc., with a freezing point of less than 100°C, or water-based polymers or emulsions with a glass transition temperature (Tg) of less than 100°C .
  • Tg glass transition temperature
  • the binder for the battery of the present invention can be prepared by a conventional method.
  • the hydrophilic monomer can exist in the form of acid or salt in water, but when it exists in the form of acid, its hydrophilic ability is low. Therefore, the adhesive for batteries of the present invention can be prepared by the following method: the monomers of the polymerization reaction are copolymerized in the water phase in the composition and form of low hydrophilicity, and the reaction product is in the form of precipitation due to insufficient hydrophilicity of the copolymer.
  • a water-dispersed slurry is formed, and the precipitate can be physically separated, and the copolymer precipitate is neutralized or hydrolyzed by adding alkali to improve the hydrophilicity of the copolymer, and the copolymer is uniformly dispersed in the water phase to obtain the battery binder.
  • carboxylic acid or sulfonic acid groups remain in the monomers of the polymerization reaction.
  • the precipitate is taken out and alkali is added to neutralize the carboxylic acid or sulfonic acid in the polymer to the corresponding carboxylic acid. Salt or sulfonate to improve its hydrophilicity, and then disperse it in the water phase.
  • the method can greatly reduce the content of residual monomers and low-molecular-weight polymers, so that the adhesive meets the requirement of less than 5% of low- and medium-molecular-weight polymers, thereby improving the cohesion and adhesion of the copolymer and other mechanical properties.
  • the following method is adopted to prepare the adhesive for batteries: add hydrophilic monomer, lipophilic monomer and water into the reaction vessel, and after heating to the reaction temperature under protective atmosphere, add The initiator initiates the reaction. After the reaction is completed, a solid-liquid mixture is obtained, the precipitate is taken, and the alkaline solution is added to neutralize the pH to 6-12 to obtain a battery adhesive, which is a transparent viscous liquid. Drying removes the moisture of the adhesive, and a solid adhesive product can be obtained.
  • reaction temperature can be selected according to different types of polymerized monomers, which can be determined by those skilled in the art through the types of monomers, types of initiators, and process conditions.
  • the additives can be added during the synthesis process, during or after neutralization by adding the lye.
  • the protective atmosphere in the present invention is an atmosphere that does not participate in the reaction, such as nitrogen, helium, neon, argon, krypton, or xenon.
  • the binder for the battery of the present invention can be used in the preparation of the battery to play a binding role, for example, in the preparation of the negative electrode sheet, the preparation of the positive electrode sheet or the preparation of the separator.
  • the battery binder is used in the preparation of lithium-ion battery pole pieces, and has high adhesion and can improve the performance of the battery.
  • the invention also provides a lithium ion battery negative electrode sheet.
  • the lithium ion battery negative electrode sheet of the present invention includes a negative electrode active material and a binder, wherein the binder is the battery binder of the present invention.
  • the negative electrode sheet of the present invention can be obtained by coating a negative electrode coating slurry on a current collector and drying it, wherein the negative electrode coating slurry includes a negative electrode active material, a conductive agent, a binder, a solvent, and the like.
  • the 90° peeling force of the negative electrode coating is ⁇ 160N/m; preferably the 90° peeling force of the negative electrode coating is 160-220N/m; more preferably the negative electrode coating
  • the 90° peeling force of the layer is 180-200 N/m.
  • the amount of the binder used in the present invention refers to the weight ratio of the solid component content of the binder to the negative electrode material and the conductive agent material in the negative electrode.
  • the negative electrode material is other than the solvent in the negative electrode coating slurry. Components, including negative active materials, conductive agents, binders, etc.
  • test method of 90° peel force in the present invention refers to ASTM D3330 of the American Society for Testing and Materials.
  • the invention also provides a lithium ion battery.
  • the lithium ion battery of the present invention includes a positive electrode, a negative electrode and an electrolyte, wherein the negative electrode is the negative electrode sheet of the lithium ion battery of the present invention.
  • the present invention also provides a battery pack, which includes a plurality of batteries according to the present invention.
  • the battery pack may include a battery module composed of multiple batteries.
  • the batteries can be connected in series or in parallel. In particular, connect them in series.
  • the hydrophilic monomers acrylic acid (AA), N-vinylpyrrolidone (NVP), acrylamide (AM) and the lipophilic monomers acrylonitrile (AN) and butyl acrylate (BA) are used in the water phase. Copolymerization to prepare a water-based binder for lithium-ion batteries.
  • the preparation method is as follows: add 5 parts of acrylamide, 8 parts of N-vinylpyrrolidone and 566 parts of distilled water into the reaction vessel, stir to dissolve, rotate at 300r/min; blow in nitrogen to drive oxygen for 30min; heat to 70°C, then add 38 parts of acrylic acid, 45 parts of acrylonitrile and 4 parts of butyl acrylate, until the temperature is constant at 70°C; then add 0.05 part of ammonium persulfate to initiate the reaction, after 9 hours of reaction, remove the precipitate, add lye to neutralize the pH to 6.5-9, The prepared transparent water-based binder for lithium ion batteries.
  • the hydrophilic monomers methacrylic acid, N-methacrylamide, and lipophilic monomers methacrylonitrile, methyl acrylate and hydroxypropyl acrylate are copolymerized in the water phase to prepare the water-based lithium ion battery. Adhesive.
  • the preparation method is as follows: add 7 parts of N-methacrylamide and 400 parts of distilled water into the reaction vessel, stir to dissolve; blow in nitrogen to drive oxygen for 30 minutes; heat to 65°C, then add 23 parts of methacrylic acid and 18 parts of acrylic acid Methyl ester, 31 parts of hydroxypropyl acrylate and 21 parts of methacrylonitrile, until the temperature rises to 65°C; then add ammonium persulfate initiator to initiate the reaction, after 22 hours of reaction, remove the precipitate, add lye to neutralize the pH to 6.5 ⁇ 9.
  • the molecular weight and molecular weight distribution were measured using the method of Example 1. Small molecules below 50,000 accounted for 0.4 wt%, low molecules below 100,000 accounted for 5 wt%, and polymers with a molecular weight above 500,000 accounted for 60 wt%.
  • the hydrophilic monomer 2-acrylamide-2-methylpropanesulfonic acid, N,N-diethylacrylamide, itaconic acid salt and the lipophilic monomer 2-ethylhexyl acrylate, Cyclohexyl methacrylate and ethyl methacrylate were copolymerized in the water phase to prepare an aqueous binder for lithium ion batteries.
  • the preparation method is as follows: add 18 parts of 2-acrylamide-2-methylpropanesulfonic acid, 22 parts of N,N-diethylacrylamide, 5 parts of itaconic acid and 400 parts of distilled water into the reaction vessel, stir to dissolve ; Then add 20 parts of 2-ethylhexyl acrylate, 12 parts of cyclohexyl methacrylate, 22 parts of ethyl methacrylate, blow in nitrogen to drive oxygen for 30 minutes; heat to 75 °C, add potassium persulfate initiator to initiate the reaction After 18 hours of reaction, the precipitate is taken out, and lye is added to neutralize the pH to 6.5-9 to prepare the water-based binder for lithium ion batteries with the above composition.
  • the molecular weight and molecular weight distribution were measured using the method of Example 1.
  • the small molecules below 50,000 accounted for 0.2% by weight, the low molecules below 100,000 accounted for 2% by weight, and the macromolecules above 500,000 accounted for 61% by weight.
  • hydrophilic monomers acrylate, 2-methacrylamide, vinyl sulfonate, and lipophilic monomers ethyl acrylate, vinyl acetate, and methacrylic acid-hydroxyethyl are copolymerized in the water phase.
  • a water-based binder for lithium-ion batteries was prepared.
  • the preparation method is: add 31 parts of acrylate, 12 parts of 2-methacrylamide, 12 parts of vinyl sulfonate and 400 parts of distilled water into the reaction vessel, stir and dissolve; then add 31 parts of ethyl acrylate and 9 parts of acetic acid Vinyl ester and 5 parts of methacrylic acid-hydroxyethyl, bubbling in nitrogen to drive oxygen for 30min; heating to 60°C, adding ammonium persulfate initiator to initiate the reaction, after reacting for 20h, take out the precipitate, add lye to neutralize the pH to 6.5 ⁇ 9.
  • the molecular weight and molecular weight distribution were measured using the method of Example 1. Small molecules below 50,000 accounted for 0.5 wt%, low molecules below 100,000 accounted for 1 wt%, and polymers with a molecular weight above 500,000 accounted for 70 wt%.
  • the hydrophilic monomer maleic acid, N-vinylpyrrolidone, N-hydroxypropyl acryl and the lipophilic monomer styrene, 2-ethylhexyl methacrylate, and hydroxypropyl methacrylate The ester is copolymerized in the water phase to prepare a water-based binder for lithium ion batteries.
  • the preparation method is as follows: add 3 parts of N-hydroxypropyl acryloyl and 400 parts of distilled water into the reaction vessel, stir to dissolve; then add 31 parts of maleic acid, 10 parts of propylene sulfonic acid, 18 parts of N-vinylpyrrolidone, 13 parts Parts of styrene, 12 parts of 2-ethylhexyl methacrylate and 13 parts of hydroxypropyl methacrylate, blow in nitrogen to drive oxygen for 30 minutes; heat to 55°C, add potassium persulfate initiator to initiate the reaction, take out after 25 hours of reaction The precipitate is added with lye to neutralize the pH to 6.5-9 to prepare the aqueous binder for lithium ion batteries with the above composition.
  • the molecular weight and molecular weight distribution were measured using the method of Example 1. Small molecules below 50,000 accounted for 0.6wt%, low molecules below 100,000 accounted for 1.4wt%, and polymers with a molecular weight of more than 500,000 accounted for 65wt% .
  • the hydrophilic monomers acrylic acid, methacrylic acid, N-hydroxyethyl acryl, propylene sulfonic acid and lipophilic monomers 2-ethylhexyl acrylate, ethyl acrylate, isobornyl methacrylate Copolymerization in the water phase to prepare a water-based binder for lithium ion batteries.
  • the preparation method is: add 8 parts of N-hydroxyethyl acryloyl, 9 parts of propylene sulfonic acid and 400 parts of distilled water into the reaction vessel, stir to dissolve; then add 13 parts of acrylic acid, 15 parts of methacrylic acid, and 30 parts of acrylic acid 2- Ethylhexyl, 15 parts of ethyl acrylate and 10 parts of isobornyl methacrylate, blow in nitrogen to drive oxygen for 30 minutes; heat to 67°C, add ammonium persulfate initiator to initiate the reaction, take out the precipitate after 23 hours of reaction, and add alkali
  • the pH of the liquid is neutralized to 6.5-9 to prepare an aqueous binder for lithium ion batteries with the above composition.
  • the molecular weight and molecular weight distribution were determined using the method of Example 1. Small molecules below 50,000 accounted for 0.2wt%, low molecules below 100,000 accounted for 4.5wt%, and polymers with a molecular weight above 500,000 accounted for 63wt% .
  • the preparation method is: add 28 parts of 2-acrylamide-2-methylpropanesulfonic acid, 32 parts of N,N-diethylacrylamide, 10 parts of itaconic acid and 400 parts of distilled water into the reaction vessel, stir to dissolve ; Then add 10 parts of 2-ethylhexyl acrylate, 12 parts of cyclohexyl methacrylate and 8 parts of ethyl methacrylate, blow in nitrogen to drive oxygen for 30min; heat to 73°C, add ammonium persulfate initiator to initiate the reaction After reacting for 19 hours, the precipitate is taken out, and lye is added to neutralize the pH to 6.5-9 to prepare the water-based binder for lithium ion batteries with the above composition.
  • the molecular weight and molecular weight distribution were determined using the method of Example 1. Small molecules below 50,000 accounted for 0.3wt%, low molecules below 100,000 accounted for 3.3wt%, and polymers with a molecular weight of more than 500,000 accounted for 66wt% .
  • the hydrophilic monomers acrylic acid (AA), N-vinylpyrrolidone (NVP), acrylamide (AM) and the lipophilic monomers acrylonitrile (AN) and butyl acrylate (BA) are in the water phase. Copolymerization to prepare a water-based binder for lithium-ion batteries.
  • the preparation method is as follows: add 5 parts of acrylamide, 8 parts of N-vinylpyrrolidone and 566 parts of distilled water into the reaction vessel, stir to dissolve at a speed of 300r/min; add 38 parts of acrylic acid, add lye to adjust the pH, and then pass in Purge oxygen with nitrogen for 30 minutes; after heating to 70°C, add 45 parts of acrylonitrile and 4 parts of butyl acrylate until the temperature is constant at 70°C; then add 0.21 part of ammonium persulfate to initiate the reaction, and add 0.21 part of ammonium persulfate every 3h The conversion is promoted, after 24 hours of reaction, lye is added to neutralize the pH to 6.5-9, and the water-based binder for lithium ion batteries with the above composition is prepared.
  • the molecular weight and molecular weight distribution were determined using the method of Example 1. The results are shown in Figure 1. Small molecules with a molecular weight of less than 50,000 accounted for 5wt%, low molecules with a molecular weight of less than 100,000 accounted for 10wt%, and high molecular weights with a molecular weight of 50w or more Molecules account for 39%.
  • the adhesive of Comparative Example 3 is the product prepared in Example 4 of Patent ZL01108511.8.
  • the hydrophilic monomers acrylic acid, N-vinylpyrrolidone, N-hydroxyethyl acryloyl and lipophilic monomers acrylonitrile and hydroxypropyl acrylate were copolymerized in the water phase to prepare a water-based adhesive for lithium ion batteries. mixture.
  • the preparation method is as follows: add 22 parts of N-hydroxyethyl acryloyl and 300 parts of distilled water to the reaction vessel, stir to dissolve; add 30 parts of acrylic acid and 15 parts of N-vinylpyrrolidone, and then blow in nitrogen to drive oxygen for a certain period of time; heating After reaching 66°C, add 25 parts of acrylonitrile and 8 parts of hydroxypropyl acrylate; then add a certain amount of potassium persulfate to initiate the reaction, take out the precipitate after 13 hours of reaction, add lye to neutralize the pH to 6.5-9, and prepare the above components Water-based binder for lithium-ion batteries.
  • the molecular weight and molecular weight distribution were determined using the method of Example 1. Small molecules below 50,000 accounted for 3.1wt%, low molecules below 100,000 accounted for 8.4wt%, and polymers with a molecular weight above 500,000 accounted for 48wt% .
  • the hydrophilic monomer 2-acrylamide-2-methylpropanesulfonic acid, acrylic acid and the lipophilic monomer 2-ethylhexyl acrylate and cyclohexyl methacrylate were copolymerized in the water phase.
  • Water-based binder for lithium ion batteries were used.
  • the preparation method is as follows: add 150 parts of distilled water, 15 parts of 2-acrylamide-2-methylpropanesulfonic acid and 5 parts of acrylic acid into the reaction vessel, add lye to adjust the pH; then add 50 parts of 2-ethylhexyl acrylate And 30 parts of cyclohexyl methacrylate, and then bubbling in nitrogen to drive oxygen for a certain period of time; after heating to 75°C, adding a certain amount of ammonium persulfate to initiate the reaction, and reacting for 17 hours to obtain the water-based binder for lithium ion batteries with the above composition.
  • the adhesive is an emulsion and needs to be used with CMC, and its performance is similar to SBR.
  • the negative pole piece was prepared, and the 90° peeling force was measured.
  • the specific methods and results are as follows:
  • Pole piece adhesion test The specific method refers to the ASTM ⁇ D3330 test method, equipment and tools: YISIDA mechanical tester (DS2-50N); 3M tape: (Scotch 600/25mm width). The specific results are shown in Table 2.
  • the preparation method of the negative pole piece is the same as that of Test Example 1.
  • the electrode prepared above and the above separator were used to prepare a battery with a specification of 406379.
  • LiPF6 lithium hexafluorophosphate

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US20230068865A1 (en) 2023-03-02
CN112662348A (zh) 2021-04-16
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